Goals'

1
Chemical Analysis II C30J

• Goals.
• To introduce students to the principles and use
  of some advanced instrumental techniques for
  detecting and quantifying analytes and to
  illustrate the importance of sampling and sample
  handling to the quality of analytical data.
• Objectives.
• To consider advanced concepts of chromatographic
  separation techniques and the detection and
  quantification of isolated analytes.
• To consider the basic principles of instrumental
  methods for the detection and quantification of
  metal ions.
• 3. To consider approaches to the collection of
  samples and methods used to assure that sample
  characteristics do not introduce systematic
  errors.
• 4. To provide opportunities to plan and
  implement an analytical approach to the
  determination of an anlayte in a real sample
  using advanced instrumental methods.
• 5. To provide opportunities for students to gain
  experience in the presentation of written and
  oral reports on analytical data and their
  interpretation.

2
Chemical Analysis II C30J
Lectures 60 Analyses of Real Samples (6
lectures) Chromatography (8 lectures) Analyses
for Metal ions (10 lectures) Final 2 hour exam
Laboratories 20 a Project to determine
analytes in a given sample
Course Test - 10 Course Assignment 10
report on the laboratory project (oral and
written)
3
Chemical Analysis II C30J

• Expectations/assumptions
• Course develops on C 10J and C 20J.
• Students have accepted responsibility for their
  own learning.
• Lectures identify the material that students are
  expected to understand and work with.
• Tutorials are sessions where students are guided
  in working with selected course material.
• Problem sheets contain questions that allow
  students to test their understanding of course
  material.
• Students do 2-3 hours of personal study per
  lecture.
• Students use the recommended text to support
  lecture notes.

4
C30J Chemical Analysis II. The Analysis of Real
Samples

• Topic 2
• Contaminants and Interferences
• Standard addition techniques.
• Methods to remove interferences

• Topic 1
• The analytical process
• The client-analyst interaction, quality, accuracy
  and precision.
• ISO 90012000
• ISO 17025
• Some definitions.

• Topic 3
• Sampling
• Errors in sampling
• Sampling protocols
• Amount of sample
• Number of samples

References Skoog, West and Holler, Fundamentals
of Analytical Chemistry, 7th edition. Miller and
Miller, Statistics for Analytical Chemistry, 3rd
edition, ISO 17025 (Library desk)
5
The Analytical Process
Client and Laboratory Manager
Quality ?
1. Problem Identification
7. Solution to the problem
2. An Hypothesis as to the cause of the problem
and an approach to test it.
6. Do the results confirm the hypothesis?
Yes
No
5. Reporting the results data, methods and
limitations. (x y) units
3. Planning the analytical work to test the
hypothesis
4. Carrying out the analyses and the Quality
Control checks
Laboratory Manager, analysts, technicians, other
lab staff
Quality ?
6
ISO 90012000
Quality fitness for purpose
Establish the quality policy quality objectives
direct control the organization to ensure
objectives are achieved.
Quality Assurance
Equipment, chemicals, facilities, personnel.
Quality Control
Quality Assessment
Problem solution
(x y) units
Analytical method
Report - (x y) units
Samples information
QA/QC/QA
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Laboratory Quality Management System The
operations or processes of the laboratory which
define its policies and objectives and the manner
in which they are implemented to ensure that the
objectives are met. eg ISO 90012000.
www.iso.org
Quality The ability of the qualitative (analyte
identification) and quantitative (accuracy,
precision) data to satisfy the requirements of
their purpose.
The QA/QC(/QA) programme The part of the
laboratory management system that focuses on the
quality of the data generated by the laboratory
Quality Assurance Documented procedures in place
within an analytical laboratory that define how
the laboratorys work is to be conducted so as to
be confident that the obtained data are of the
required quality. QA consists of quality control
and quality assessment activities.
Quality Control The practices and procedures
that lead to the achievement of quality
analytical data (suitable facilities, staff
competence and training, good laboratory
practices, standard operating and reporting
procedures).
Quality Assessment The practices and the data
generated by them that illustrate that the QC
activities have been effected and that the data
generated are of the quality required (SRMs,
spiking, replicates, inter-laboratory
comparisons, control charts, auditing,
statistical analyses).
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ISO 17025 General Requirements for the
competence of testing and calibration laboratories

• Scope
• 1.1 applies to all laboratories (not just
  chemical) regardless of size.
• 1.4 this international standard is for use by
  laboratories in developing their quality,
  administrative and technical systems that govern
  their operations. Laboratory clients,
  regulatory authorities and accreditation bodies
  may also use it in confirming or recognizing the
  competence of laboratories.

• Normative references
• Terms and definitions
• Refer to ISO 90011994 , 90021994 and ISO/IEC
  Guide 2,
• These have now been incorporated into ISO
  90002000, ISO 90012000.

9
ISO 17025 General Requirements for the
competence of testing and calibration
laboratories (cont.)

• Management requirements
• 4.1 Organization
• The laboratory shall (amongst other things)
• be legally responsible
• operate a management system covering work in the
  laboratories permanent facility and at sites
  away from its permanent facility (if relevant)
• have technical management with responsibility
  for the technical operations and the provision of
  resources
• have a quality manager with defined
  responsibility and authority for ensuring that
  the quality system is implemented and followed at
  all times

4.2 Quality System The laboratory shall
(amongst other things) establish, implement
and maintain a quality system (like
ISO90012000) document its policies, systems,
programmes, procedures and instructions the
quality system policies, and objectives shall be
defined in a quality manual include
technical procedures.
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ISO 17025 General Requirements for the
competence of testing and calibration
laboratories (management requirements cont.)
4.3 Document Control 4.4 Review of requests,
tenders and contracts 4.5 Subcontracting of
tests and calibrations 4.6 Purchasing (chemical
and instrument quality, inventories) 4.7
Service to client 4.8 Complaints
4.9 Control of nonconforming testing and/or
calibration work (quality control charts, RMs,
standard additions, instrument calibrations,
) 4.10 Corrective action 4.11 Preventative
action
4.12 Control of records 4.13 Internal audits
4.14 Management reviews
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ISO 17025 General Requirements for the
competence of testing and calibration
laboratories (cont.)
5. Technical requirements 5.1 General 5.1.1
Many factors determine the correctness and
reliability of the test and/or calibrations
performed by a laboratory. These factors include
contributions from human factors, accommodation
and environmental conditions, test and
calibration methods and method validations,
equipment, measurement traceability, sampling
and handling of test and calibration items. The
laboratory shall take into account these factors
in developing tests and calibration procedures ,
in training and qualification of personnel, and
in the selection and calibration of the equipment
it uses.
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ISO 17025 General Requirements for the
competence of testing and calibration
laboratories. (technical requirements cont.)
5.2 Personnel (competence, training, job
descriptions, responsibilities) 5.3
Accommodation and environmental conditions
(permanent and in the field, sterility , dust,
temperature, vapors, access, )
5.4 Test and calibration methods and method
validation shall use appropriate methods
and procedures including sampling, handling,
transport, storage and preparation of items to be
tested . shall use test and/or calibration
methods, including methods of sampling, which
meet the needs of the client and which are
appropriate Methods published in
international, regional or national standards
shall preferably be used. shall confirm
(verify) that it can properly operate standard
methods before introducing the tests or
calibrations. Methods developed shall have
been validated appropriately before use.
shall have and shall apply procedures for
estimating uncertainty of measurement.
(duplicates, replicates)
13
ISO 17025 General Requirements for the
competence of testing and calibration
laboratories. (technical requirements cont.)
5.5 Equipment (scope, operation, maintenance,
calibration) 5.6 Measurement traceability
(calibrations to international standards sample
to result reference standards and
materials) 5.7 Sampling shall have a
sampling plan and procedures for sampling
sampling plans shall, whenever reasonable, be
based on appropriate statistical methods. 5.8
Handling of test and calibration items
(transportation, preservation, storage). 5.9
Assuring the quality of test and calibration
results 5.10 Reporting the results
Appendices and bibliography. (see copy in
library)